Assessment of robustness on analysis using headspace solid-phase microextraction and comprehensive two-dimensional gas chromatography through experimental designs

• Published in: Talanta (Oxford) Vol. 129; pp. 303 - 308
• Main Authors: Oliveira, Luciana F., Braga, Soraia C.G.N., Filgueiras, Paulo R., Augusto, Fabio, Poppi, Ronei J.
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 01.11.2014
• Subjects: Chocolate; Comprehensive two-dimensional gas chromatography; Plackett–Burman design; Robustness; Volatiles; Chocolate; Plackett–Burman design; Robustness; Comprehensive two-dimensional gas chromatography; Volatiles
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2014.05.038

Plackett–Burman experimental design was applied for the robustness assessment of GC×GC–qMS (Comprehensive Two-Dimensional Gas Chromatography with Fast Quadrupolar Mass Spectrometric Detection) in quantitative and qualitative analysis of volatiles compounds from chocolate samples isolated by headspace solid-phase microextraction (HS-SPME). The influence of small changes around the nominal level of six factors deemed as important on peak areas (carrier gas flow rate, modulation period, temperature of ionic source, MS photomultiplier power, injector temperature and interface temperature) and of four factors considered as potentially influential on spectral quality (minimum and maximum limits of the scanned mass ranges, ions source temperature and photomultiplier power). The analytes selected for the study were 2,3,5-trimethylpyrazine, 2-octanone, octanal, 2-pentyl-furan, 2,3,5,6-tetramethylpyrazine, and 2-nonanone e nonanal. The factors pointed out as important on the robustness of the system were photomultiplier power for quantitative analysis and lower limit of mass scanning range for qualitative analysis. [Display omitted] •Experimental design was applied for the assessment of robustness of GC×GC–qMS.•Analysis of volatiles compounds from chocolate samples isolated by HS-SPME.•Half-normal probability plots, error analysis and permutation tests were employed for model interpretation.•Factor significant to the robustness in quantitative analysis was the photomultiplier power.•Factor significant to the robustness in qualitative analysis was the lower limit of mass scanning range.